2-acetylpyrazine continuous recrystallization device and method and application thereof

A technology of acetylpyrazine and crystallization device, applied in the field of 2-acetylpyrazine continuous recrystallization device, can solve problems such as low production efficiency, low yield, safety and environmental protection risks and the like

Active Publication Date: 2021-11-30
JINAN ENLIGHTEN BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem of low utilization rate of 2-acetylpyrazine in the 2-acetylpyrazine recrystallization method existing in the prior art, resulting in low yield, low production efficiency and safety and environmental protection risks caused by batch operation Problem, the present invention proposes a 2-acetylpyrazine continuous recrystallization device and its method and application, by setting three feeding ports in the crystallizer, the inlet of the mixed solution containing 2-acetylpyrazine is located above the solvent, When the solution in the crystallizer flows from bottom to top like this, as the temperature decreases step by step, the crystallization of 2-acetylpyrazine falls back to the bottom of the crystallizer, because at the position of the mixed solution inlet lower than 2-acetylpyrazine The purity of the solvent is high, so it helps 2-acetylpyrazine to maintain a crystalline state, and it can also prevent 2-acetylpyrazine crystals from being doped with uncrystallized components, which will affect the purity of 2-acetylpyrazine crystallization products

Method used

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  • 2-acetylpyrazine continuous recrystallization device and method and application thereof

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Experimental program
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Embodiment 1

[0080] Such as figure 1 As shown, it is a 2-acetylpyrazine continuous recrystallization device disclosed in this embodiment:

[0081] The dissolution device 1, crude product transfer pump 2, decolorization device a7 or decolorization device b8, turnover tank 9, feed pump 3, crystallizer 10, slurry pump 4, filter a11 or filter b12, reuse mother liquor tank 14 , Recycling mother liquor pump 5 is sequentially connected through pipelines, and crystallizer 10 is sequentially connected with mother liquor tank 13 and mother liquor pump 6 through second discharge port 19 through pipelines to form a continuous recrystallization production line.

[0082] The crystallizer 10 is provided with six sections from bottom to top, the lower temperature is higher than the upper temperature, the first feed port 15 is located in the fourth section, the second feed port 16 is located in the second section, and the third feed port 17 is located in the second section. In the first section, the first...

Embodiment 2

[0093] The specific steps for the continuous recrystallization of 2-acetylpyrazine using the device described in Example 1 are as follows:

[0094] Step ①: Put 1056kg of crude 2-acetylpyrazine into the dissolving device 1, and set the cumulative feed amount of the solvent to 8m 3 , the solvent is automatically metered by the flowmeter and added to the dissolving device; set the temperature of the kettle to 47°C, then open the jacketed hot water inlet regulating valve of the dissolving device 1, and start heating until the crude 2-acetylpyrazine is completely dissolved to solvent, and stabilized at around 47°C.

[0095] Step ②: Open the hot water inlet and outlet valves of the jacket of decolorizing device a7 or decolorizing device b8 and turnover tank 9, and feed hot water at 50°C to maintain the internal temperature of decolorizing device a7 or decolorizing device b8 and turnover tank 9 at 45 ~50°C; set the feed flow rate of the crude product solution to 500L / h, the dissolve...

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Abstract

The invention relates to the field of chemical component purification, and in particular, relates to a 2-acetylpyrazine continuous recrystallization device and method and an application of the device. For solving the problems of low yield caused by low utilization rate of 2-acetylpyrazine and low production efficiency and safety and environmental protection risks caused by intermittent operation in a 2-acetylpyrazine recrystallization method in the prior art, the invention provides the 2-acetylpyrazine continuous recrystallization device and method and the application of the device. A crystallizer is provided with three feed ports, an inlet of a mixed solution containing 2-acetylpyrazine is located above a solvent, 2-acetylpyrazine is crystallized and falls back to the bottom of the crystallizer, and the situation that 2-acetylpyrazine crystals are doped with uncrystallized components, and the purity of 2-acetylpyrazine crystallized products is affected is avoided. Two discharge holes are formed in the upper part and the bottom of the crystallizer, so that solutions with different components can be obtained and are reused after being subjected to different treatments, and continuous recrystallization of 2-acetylpyrazine is realized.

Description

technical field [0001] The invention relates to the field of chemical component purification, in particular to a 2-acetylpyrazine continuous recrystallization device and its method and application. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] In the field of chemical synthesis or pharmaceutical production, a variety of components or intermediate products will be obtained. Among them, 2-acetylpyrazine is an important organic synthesis intermediate. In addition to being used as a spice in the food industry, it is also an important pharmaceutical intermediate. It is widely used in the synthesis of anti-malarial, anti-tumor, anti-bacterial, and anti-viral and drugs for pa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/12
CPCC07D241/12
Inventor 卢朋朱振峰贺文良李晟
Owner JINAN ENLIGHTEN BIOTECH CO LTD
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